US4996108A - Sheets of transition metal dichalcogenides - Google Patents
Sheets of transition metal dichalcogenides Download PDFInfo
- Publication number
- US4996108A US4996108A US07/297,464 US29746489A US4996108A US 4996108 A US4996108 A US 4996108A US 29746489 A US29746489 A US 29746489A US 4996108 A US4996108 A US 4996108A
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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 21
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 100
- 239000007788 liquid Substances 0.000 claims abstract description 61
- 239000000203 mixture Substances 0.000 claims abstract description 43
- 239000000725 suspension Substances 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000000839 emulsion Substances 0.000 claims abstract description 7
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 7
- 239000011669 selenium Substances 0.000 claims abstract description 7
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 7
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 6
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 6
- 239000010955 niobium Substances 0.000 claims abstract description 6
- 239000011593 sulfur Substances 0.000 claims abstract description 6
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 6
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011733 molybdenum Substances 0.000 claims abstract description 5
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 5
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000010937 tungsten Substances 0.000 claims abstract description 5
- 229910052798 chalcogen Inorganic materials 0.000 claims abstract description 4
- 150000001787 chalcogens Chemical group 0.000 claims abstract description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 96
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 95
- 238000000034 method Methods 0.000 claims description 62
- 239000010410 layer Substances 0.000 claims description 53
- 239000000758 substrate Substances 0.000 claims description 37
- 230000008569 process Effects 0.000 claims description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 24
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 19
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 18
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 claims description 14
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 12
- 239000002356 single layer Substances 0.000 claims description 11
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 10
- WDECIBYCCFPHNR-UHFFFAOYSA-N chrysene Chemical compound C1=CC=CC2=CC=C3C4=CC=CC=C4C=CC3=C21 WDECIBYCCFPHNR-UHFFFAOYSA-N 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 6
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 4
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 claims description 3
- 229940035429 isobutyl alcohol Drugs 0.000 claims description 3
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 3
- 229940037312 stearamide Drugs 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- YTZKOQUCBOVLHL-UHFFFAOYSA-N tert-butylbenzene Chemical compound CC(C)(C)C1=CC=CC=C1 YTZKOQUCBOVLHL-UHFFFAOYSA-N 0.000 claims description 3
- ABDKAPXRBAPSQN-UHFFFAOYSA-N veratrole Chemical compound COC1=CC=CC=C1OC ABDKAPXRBAPSQN-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 2
- 239000011368 organic material Substances 0.000 claims description 2
- GWHJZXXIDMPWGX-UHFFFAOYSA-N 1,2,4-trimethylbenzene Chemical compound CC1=CC=C(C)C(C)=C1 GWHJZXXIDMPWGX-UHFFFAOYSA-N 0.000 claims 2
- UTLXUGOVTIJBAP-UHFFFAOYSA-N cyclopenta-1,3-diene 5-(2-cyclopenta-2,4-dien-1-ylethyl)cyclopenta-1,3-diene iron(2+) Chemical compound [Fe++].[Fe++].c1cc[cH-]c1.c1cc[cH-]c1.C(C[c-]1cccc1)[c-]1cccc1 UTLXUGOVTIJBAP-UHFFFAOYSA-N 0.000 claims 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims 1
- 230000002378 acidificating effect Effects 0.000 claims 1
- WIRUZQNBHNAMAB-UHFFFAOYSA-N benzene;cyclohexane Chemical compound C1CCCCC1.C1=CC=CC=C1 WIRUZQNBHNAMAB-UHFFFAOYSA-N 0.000 claims 1
- VVUBWCWVDFCEOP-UHFFFAOYSA-N benzene;styrene Chemical compound C1=CC=CC=C1.C=CC1=CC=CC=C1 VVUBWCWVDFCEOP-UHFFFAOYSA-N 0.000 claims 1
- 229910001338 liquidmetal Inorganic materials 0.000 claims 1
- FYGHSUNMUKGBRK-UHFFFAOYSA-N trimethylbenzene Natural products CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 claims 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims 1
- 239000010408 film Substances 0.000 description 104
- 229910052961 molybdenite Inorganic materials 0.000 description 23
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 18
- 239000011521 glass Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 7
- 238000003892 spreading Methods 0.000 description 7
- 230000007480 spreading Effects 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 150000001336 alkenes Chemical class 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000005357 flat glass Substances 0.000 description 5
- 230000005484 gravity Effects 0.000 description 5
- 230000002209 hydrophobic effect Effects 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- -1 1-chloronaphthelene Chemical compound 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 239000004793 Polystyrene Substances 0.000 description 3
- 229910004211 TaS2 Inorganic materials 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 239000007900 aqueous suspension Substances 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229920002223 polystyrene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- AUHZEENZYGFFBQ-UHFFFAOYSA-N 1,3,5-trimethylbenzene Chemical compound CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 2
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 2
- 229910020042 NbS2 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 2
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 description 1
- JTPNRXUCIXHOKM-UHFFFAOYSA-N 1-chloronaphthalene Chemical compound C1=CC=C2C(Cl)=CC=CC2=C1 JTPNRXUCIXHOKM-UHFFFAOYSA-N 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 1
- 229910017147 Fe(CO)5 Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- KEHVDLIJTZDRLL-UHFFFAOYSA-N hex-1-ene octadecanamide Chemical compound C(CCCCCCCCCCCCCCCCC)(=O)N.C=CCCCC KEHVDLIJTZDRLL-UHFFFAOYSA-N 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/20—Two-dimensional structures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/78—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by stacking-plane distances or stacking sequences
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
- C03C2217/287—Chalcogenides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
Definitions
- This invention relates to sheets or films of transition metal dichalcogenides, particularly molybdenum disulfide.
- an amorphous transition metal dichalcogenide product is prepared by low temperature non-aqueous precipitation of the compound from mixtures of the metal salts.
- the amorphous products are converted into sheets of metal dichalcogenides referred to in the patent as having a "rag-like" structure by controlled heating at temperatures between 250° and 400° C.
- neither the end product, nor the intermediate product are oriented films or sheets, that is films or sheets wherein the crystalline c-axes of single layers of the metal dichalcogenide are aligned.
- U.S. Pat. No. 4,647,386 to Jamieson discloses an intercalated transition metal based solid lubricating composition.
- a transition metal dichalcogenide is intercalated with a metal, preferably a coinage metal.
- the invention provides a process for forming sheet-like compositions of the formula MX 2 :Y, wherein MX 2 is a layer-type transition metal dichalcogenide, M is a metal selected from the group consisting of niobium, tantalum, molybdenum and tungsten, X is a chalcogen selected from the sulfur and selenium and Y is a material located between layers of MX 2 .
- the process includes the steps of forming a suspension of the MX 2 in water and adding a liquid which is immiscible with water to the suspension to form a mixture. The mixture is agitated to form a temporary emulsion. The emulsion is allowed to rest until the water and the liquid separate with an interface therebetween.
- a sheet-like composition of MX 2 :Y forms at the interface.
- MX 2 has a crystalline structure with c-axes aligned in a direction perpendicular to the plane of the layers.
- the MX 2 suspension comprises exfoliated layers of MX 2 .
- the composition then comprises one molecular thickness layers of the MX 2 . These layers may be separated by molecules of the water immiscible liquid, water molecules or molecules of a foreign substance dissolved in the liquid.
- the invention also relates to compositions prepared according to the processes described above.
- the compositions maY be used to coat objects.
- the invention provides thin, aligned sheets or films and coatings of transition metal dichalcogenides by a relatively expeditious process which can be readily scaled to provide large area films and coatings.
- These coatings or films have unique qualities.
- such thin, oriented films of molybdenum disulfide have unique optical qualities and can be used as selective filters. These films are believed to have advantageous lubrication qualities when compared with non-oriented films.
- the invention may be used to make relatively inexpensive, large area energy selective X-ray focusing devices.
- the invention also provides unique layered compositions which may be utilized for the composition of the transition metal dichalcogenide, for the properties of other substances between layers of the metal dichalcogenides or combinations of the two.
- the optical properties of MoS 2 in combination with the other organic molecules between MoS 2 layers can be used as selective optical filters.
- FIG. 1a is a diagrammatic representation of a process for making a thin, oriented film of a transition metal dichalcogenide according to an embodiment of the invention and employing a water immiscible liquid having a specific gravity less than 1;
- FIG. 1b is a view similar to FIG. 1a showing the process using a water immiscible liquid with a specific gravity greater than 1;
- FIG. 2 is an enlarged view of the portion within the circle in FIG. 1a;
- FIG. 3a is a diagrammatic representation of the coating of an object with a film produced by the process of FIG. 1b;
- FIG. 3b is a diagrammatic representation of the process of coating of a wet glass slide employing the film produced by the process of FIG. 1b;
- FIG. 4 is an enlarged, diagrammatic representation of a portion of an object coated with a film of transition metal dichalcogenide incorporating water immiscible liquid and water molecules produced by the processes FIGS. 3a or 3b;
- FIG. 5 is a view similar to FIG. 4 showing the object and film after heating
- FIG. 6 is a diagrammatic side view of the metal dichalcogenide film shown after drying
- FIG. 7 is an enlarged view of the portion within a circle of FIG. 6 showing ferrocene between the layers of metal dichalcogenide;
- FIG. 8 is an enlarged diagrammatic view of an object coated with a film of transition metal dichalcogenide incorporating ferrocene shown after baking;
- FIG. 9 is a diagrammatic view of a method for coating a hydrophobic substrate with molybdenum disulfide film
- FIG. 10 is a diagrammatic view of a process for transferring a molybdenum disulfide film from one substrate to another;
- FIG. 11a is a proposed model of single layers of molybdenum disulfide in water
- FIG. 11b is a view similar to FIG. 11a and showing the layers as modified by the presence of a water immiscible liquid;
- FIG. 12 is an SEM micrograph of a spread film of exfoliated molybdenum disulfide
- FIG. 13 is a graph of the x-ray diffraction patterns of a film of un-exfoliated MoS 2 powder prepared by
- FIG. 14 is a graph of the x-ray diffraction patterns of a film of exfoliated molybdenum disulfide showing the film on a flat glass substrate deposited using hexene
- FIG. 15 is a graph of the x-ray diffraction pattern of a film of exfoliated MoS 2 on a flat glass substrate, with ferrocene included between the MoS 2 layers;
- FIG. 16 is a diagram of optical absorption for
- a process for preparing single layers of molybdenum disulfide in water is described in detail in pending U.S. patent application Ser. No. 855,517.
- the process involves exfoliating a lithium intercalated layered transition metal dichalcogenide, such as MoS 2 , TaS 2 , NbS 2 or WS 2 by immersion in water.
- Selenium may replace the sulfur as the dichalcogen.
- molybdenum disulfide powder was soaked in a solution of n-butyl lithium in hexane for about 48 hours in a dry box containing an argon atmosphere. Once the molYbdenum disulfide was fully intercalated with lithium ions between the layers of molybdenum disulfide, the product was removed and washed repeatedly in hexane, dried and sealed in a vial while still in the dry box under argon atmosphere. The vial was then removed from the dry box, immersed in water, and the cap removed from the vial. Upon contact of the contents of the vial with liquid water, copious gas evolution followed and the molybdenum disulfide powder formed a highly opaque suspension in the water.
- the suspension was agitated, in this case ultrasonicated, during the reaction to assist in the exfoliation.
- the hydrogen gas produced by the reaction between the lithium and the water pushed the layers of molybdenum disulfide apart until they were completely separated.
- the suspension was repeatedly centrifuged and washed with distilled water. A final concentration of molybdenum disulfide of about 5 mg/cc of water was produced.
- a liquid 21 is immiscible with water and, in this case, has a density less than water.
- organic solvents were tested including alkanes, alkenes and butyl alcohol (n-butyl and iso-butyl).
- iron pentacarbonyl was also used as the immiscible liquid.
- the liquid was added to the suspension of molybdenum disulfide in water to form a two-phase liquid 23. The suspended molybdenum disulfide stays in the water.
- the mixture was then shaken as indicated by arrows 25 and formed an unstable emulsion containing globules of water in the liquid.
- the molybdenum disulfide layers placed themselves at the surfaces of the resulting globules of water. When the shaking ceased, these globules gradually migrated towards the water/liquid interface 27 where they coalesced with each other.
- the molybdenum disulfide molecular layers formed a film at the horizontal interface 27 between the two liquids. With moderate shaking, both the water and the water immiscible liquid became clear. Therefore, all of the molybdenum disulfide was in the interface film as shown to the right of FIG. 1a. Clear water 20.1 remained below the film.
- FIG. 1b illustrates a variation of the process of FIG. 1a wherein the specific gravity of the water immiscible liquid is greater than 1.
- Suitable solvents tested were 1,2-dichloroethane, carbon tetrachloride, dimethoxybenzene, 1-chloronaphthelene, and iron pentacarbonyl.
- the solvent 22 was mixed with the molybdenum disulfide suspension to form a two-phase liquid 24 which is agitated as indicated by arrows 26. Film accumulation occurred both at water/liquid interface 28 as well as at water/air interface 30. However, it was found that mercury does not work.
- FIG. 11a this shows one of the single layers of molybdenum disulfide 32 contained within the water suspension 20 of FIGS. 1a and 1b. While we do not wish to be bound to this theory, it is believed that each of the single layers 20 possesses a net negative charge due to surface hydration represented in FIG. 11a by the OH - ions. There are several indications of this.
- the exfoliated molybdenum disulfide particles show a net drift towards the anode in an electrophoresis apparatus when a voltage is applied across the electrodes.
- FIG. 11b this shows the result of mixing an aqueous suspension of exfoliated molybdenum disulfide with a liquid which is immiscible with water and agitating the resulting mixture as described above. It is suggested that shaking brings the immiscible liquid in ready contact with the hydrated particles of molybdenum disulfide and this induces displacement of the hydroxyl ions adsorbed on the basal planes by the liquid molecules. At the basal planes, the hydroxyl ions presumably are more loosely bound and are therefore easily displaced. Therefore, the basal regions of the particles are covered by immiscible liquid and the edge regions by the hydroxyl ions as shown in FIG. 11b.
- the first configuration that forms after agitating the two-phase mixture is that of globules encased by molybdenum disulfide layers. These globules are inherently unstable and, in time, coalesce, presumably because the free energy associated with the globules is much higher (proportional to interfacial area of the globules) than that of the final phase-separated mixture with a single horizontal interface between the water and the water immiscible liquid. With the coalescence of globules, the modified single layers of FIG. 11b form a multi layer membrane at the interface. Referring to FIG. 2, this shows in diagrammatic form an enlarged section through the membrane.
- the layers 32 of molybdenum disulfide are stacked on each other with water molecules 34, identified by while ovals, and liquid molecules 36, identified by black ovals, trapped between them. Based on the above discussion, it can be expected that the immiscible liquid will be non-polar or weakly polar.
- the molybdenum disulfide film at the interface has a tendency to spread. As shown in FIGS. 1a and 1b, the film 32 tends to creep along the walls of a glass container holding the mixture.
- the thin film of molybdenum disulfide spreads as a thin layer on wetted surfaces.
- a pre-cleaned glass slide 38 was wetted after a brief wash with dilute hydrofluoric acid and then dipped into the phase separated mixture such that the lower end just touched the accumulated molybdenum disulfide at the interface of water 20.1 and solvent 21.
- the slide was withdrawn from solution and was kept hanging vertically in room air for drying.
- the film was apparently dry after a few minutes, it was not completely devoid of water at this stage. However, the resulting film was optically very uniform and highly oriented as determined by x-ray diffraction.
- the diffraction patterns of the spread films of exfoliated molybdenum disulfide have only one prominent peak, identified as the (001) line, corresponding to a c-spacing of 6.2 angstroms.
- the lack of other lines suggests that the film consists of the layers with nearly parallel c-axes. In other words, the c-axes of the molybdenum disulfide were substantially parallel and perpendicular to the immediately underlying surface of the substrate.
- Films of molybdenum disulfide were grown on various hydrophilic substrates using this method including glass, ceramics, oxidized copper, oxidized silicon, tungsten trioxide, glass and even cardboard.
- a slight variation of the above method is to dip a dry hydrophilic substrate into the phase-separated mixture past the accumulated molybdenum disulfide into the water 20.1.
- the film was not formed when inserting the glass substrate through the interface 27 into the water 20.1, but a film of molybdenum disulfide was deposited when the substrate, now wet, was withdrawn.
- Another method of depositing films tested was to allow the water immiscible liquid to evaporate after the process of FIG. 1a, leaving the molybdenum disulfide film at the air/water interface as shown in FIG. 9.
- the resulting multi-layer film 32 can be transferred to a hydrophobic substrate 33 by simply touching the film with the substrate oriented horizontally, alternatively from above the film 32 disulfide interface and from below the film 32.
- FIG. 10 illustrates another method used for coating hydrophobic surfaces with film.
- the film 52 disengaged itself from the glass slide and re-spread on the air/water interface 54.
- the hydrophobic substrate 56 was placed on a support 58 in a horizontal position just under the air/water interface 54.
- the water level was then lowered past the substrate and the film is deposited on a non-polar substrate as shown to the right of the figure.
- the proportion of the film transferred was directly related to the fraction of the slide which was immersed in water.
- the substrate 56 with the newly transferred film of molybdenum disulfide 60 was then removed from the container and let dry in room air.
- FIG. 3a illustrates a further method of transferring films when the water immiscible liquid has a specific gravity greater than 1 as previously used in the process of FIG. 1a.
- the film was deposited directly on to a metal substrate.
- FreshlY etched metals including aluminum, copper or steel 64 were inserted into the water/air interface 30.
- a coating of molybdenum disulfide was deposited on them. This method could be useful for preparing lubricant coatings on metal surfaces, for example.
- styrene was used as the water immiscible liquid to obtain styrene molecules between the MoS 2 , layers giving a c-spacing of 11.5 angstroms.
- the composition was subsequentlY heated to about 60° C. in an inertaargon atmosphere to polymerize the styrene into polystyrene. This may be of use in protecting the MoS 2 , layers.
- ferrocene was dissolved in benzene and, alternatively in, carbon tetrachloride to produce films shown in FIGS. 7 and 8 that included ferrocene 76 between the molybdenum disulfide layers 74.
- the resulting films are highly oriented as shown by x-ray diffraction. The orientation is much better than obtained with organic solvent alone. Additionally, the presence of ferrocene between the layers makes the resultant films on substrates electrically more conducting.
- the water 20.1 was decanted and the water immiscible liquid 22 was pipetted.
- the liquid 21 was evaporated and the water 20.1 pipetted.
- the resultant composition was dried in room air.
- the result was a powder 72 of molybdenum disulfide as shown in FIG. 6.
- the enlarged view of FIG. 7 shows that the powder includes a plurality of layers 74 of MoS 2 with molecules 76 of ferrocene, represented by x's, between the layers
- the resultant composition can be identified by the formula MX 2 :Y, where Y is the ferrocene. This was in powder form.
- FIG. 8 shows a molybdenum disulfide film incorporating ferrocene molecules coating a substrate 78 via the processes described above. It should be noted that there is only a single layer of ferrocene molecules between the layers of molybdenum disulfide instead of two layers of liquid molecules as shown in FIG. 2.
- CuPc copper phthalocyanine
- Pc phthalocyanine
- stearamide stearamide
- chrysene a solute dissolved in the solvent.
- FIG. 12 is a SEM micrograph of a film obtained from a suspension of exfoliated molybdenum disulfide prepared using 1-hexene as the water immiscible liquid.
- the thickness of the films prepared ranged from 30 angstroms to a few microns, the thickness being measured by various techniques.
- the thickness of the spread films can be somewhat controlled by the concentration of the initial molybdenum disulfide suspension. Higher values were measured by interference fringe method using a Wild (T. M.) model M20 interference microscope with a narrow band-pass filtre at 550 nm.
- this method showed that the measured films were of high optical quality with the observed fringe patterns were straight and devoid of any other observable structure on the entire surface area.
- a Perkin-Elmer (T. M.) Model 595 scanning Auger microprobe (SAM) was used to provide depth profiles of thin films. Samples measured by this technique showed thicknesses down to about 30 angstroms.
- FIG. 13 shows x-ray diffraction patterns for films spread on glass obtained using a Philips (T. M.) diffractometer using nickel-filtered Cu cc K radiation.
- FIG. 13(a). shows a diffraction pattern for film prepared from as-received MoS 2 powder.
- FIG. 13(b) is for film of unexfoliated molybdenum disulfide deposited on glass by the method of spreading using 1-hexene.
- the resulting film is seen to be highly oriented in that the crystallites of the film are placed on the substrate such that all basal planes are parallel to each other. This is indicated by the fact that only (001) lines are present in the diffraction pattern while the (100) and (110) lines are absent.
- FIG. 13 shows x-ray diffraction patterns for films spread on glass obtained using a Philips (T. M.) diffractometer using nickel-filtered Cu cc K radiation.
- FIG. 13(a). shows a diffraction pattern for
- 13(c) shows a diffraction pattern obtained after transferring the same film to another glass substrate via a clean water surface using the transferring technique shown in FIG. 10.
- the identical x-ray diffraction patterns suggest that the transfer has introduced no major disruptions in the orientation of the film.
- FIG. 14 shows a sequence of x-ray diffraction patterns for a film of exfoliated molybdenum disulfide on a flat glass substrate prepared using the interface between n-butyl alcohol and water, baked at various temperatures in a flow of pre-purified argon. It was observed that baking at increasingly higher temperatures in an inert atmosphere sharpened the (001) peak. The higher orders are not seen and are most probably are buried in the signal from the substrate as is usual for a thin film. The broad hump around 23° is due to the substrate.
- FIG. 15 shows an x-ray diffractogram of a film of exfoliated MoS 2 on a flat glass substrate prepared by using the interface between a solution of ferrocene in C 6 H 6 and water. Three peaks identified as (001), (002) and (003) with a c-spacing of 11.8 angstroms indicated that a monolayer of ferrocene is included between the layers of MoS 2 .
- FIG. 16 shows optical absorption spectra of films obtained using an Oriel monochromator and detector.
- Curve “a” is the absorption spectra of a suspension of fine MoS 2 crystallites in water showing the true characteristic exciton peaks labelled "A" and "B".
- the curve marked “b” is of a film of exfoliated molybdenum disulfide on a flat glass substrate.
- Curve “c” is that of the same film after heating to 300° C. for 15 minutes in an argon atmosphere.
- the spreading techniques for coating substrates with films is believed to be the result of a surface tension gradient. This results from attractive forces between hydroxyl groups at the edge sites of the molybdenum disulfide layers and a thin layer of water on the glass slide or other hydrophilic materials.
- the cohesive forces between the water immiscible liquid molecules adsorbed on the basal planes of the molybdenum disulfide and the molecules of the hydrophobic substrates are believed to be responsible for spreading films on PTFE, polystyrene and the like.
- the surface tension model also seems to account for the observation that while the films of molybdenum disulfides spontaneously spread on wet slide from the alkane/water and 1-hexene/water interfaces, they do not spread from an alcohol/water interface. The reason for the above difference may lie with a vastly different interfacial tension of the two liquid/water systems.
- optical uniformity and high orientation in the spread films make them very attractive considering the simplicity in preparation.
- the fact that good quality films can be obtained on a variety of substrates even with unexfoliated, as-received material in the form of a powder is also of interest.
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Abstract
Description
______________________________________ Solvent Solute Properties and Uses ______________________________________ 1. benzene, ferrocene Highly oriented, and carbon better electrical tetrachloride conductivity. Powder may have applications as a catalytic material. 2. benzene, Phthalocyanine Blue color films, hexene dyes, CuPc, possible gas sensing Pc etc. ability. 1-chlorona- phthalene 3. benzene, chrysene whitish film, hexene fluorescent film, purple fluorescence upon exposure to ultra-violet radiation. 4. hexene stearamide widely separated MoS.sub.2 layers. ______________________________________
Claims (26)
MX.sub.2 :Y
MX.sub.2 :Y
MX.sub.2 :Y
MX.sub.2 :Y
Priority Applications (5)
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US07/297,464 US4996108A (en) | 1989-01-17 | 1989-01-17 | Sheets of transition metal dichalcogenides |
AU47013/89A AU630394B2 (en) | 1989-01-17 | 1989-12-19 | Sheets of transition metal dischalcogenides |
EP19900300290 EP0382339A1 (en) | 1989-01-17 | 1990-01-10 | Sheets of transition metal dichalcogenides |
KR1019900000644A KR900011670A (en) | 1989-01-17 | 1990-01-17 | Sheet of Transition Metal Decalcogenide |
JP807190A JP2930344B2 (en) | 1989-01-17 | 1990-01-17 | Layered transition metal dichalcogenide and method for producing the same |
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US07/297,464 US4996108A (en) | 1989-01-17 | 1989-01-17 | Sheets of transition metal dichalcogenides |
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EP (1) | EP0382339A1 (en) |
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EP0382339A1 (en) | 1990-08-16 |
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JP2930344B2 (en) | 1999-08-03 |
AU630394B2 (en) | 1992-10-29 |
KR900011670A (en) | 1990-08-01 |
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